CN114768721A - Device and method for preparing lithium battery positive electrode material precursors with various particle sizes - Google Patents

Device and method for preparing lithium battery positive electrode material precursors with various particle sizes Download PDF

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Publication number
CN114768721A
CN114768721A CN202210368758.5A CN202210368758A CN114768721A CN 114768721 A CN114768721 A CN 114768721A CN 202210368758 A CN202210368758 A CN 202210368758A CN 114768721 A CN114768721 A CN 114768721A
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lithium battery
positive electrode
electrode material
battery positive
driving motor
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CN114768721B (en
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李少龙
米玺学
王耀玺
孙磊
郭淑珍
吴靖
杨永生
王鹏
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Ningxia Medium Color New Materials Co ltd
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Ningxia Zhongse Jinhui New Energy Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/006—Baffles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/0066—Stirrers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00761—Details of the reactor
    • B01J2219/00763—Baffles
    • B01J2219/00765—Baffles attached to the reactor wall
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides a device and a method for preparing lithium battery positive electrode material precursors with various particle sizes, and belongs to the technical field of lithium battery positive electrode material production. The device comprises a reaction kettle, a stirring mechanism and a baffle mechanism. The stirring mechanism is arranged in the reaction kettle and comprises a driving motor, a stirring shaft connected to the output end of the driving motor and at least one blade component arranged on the stirring shaft. The drive motor can rotate in the forward direction and also can rotate in the reverse direction. At least one of the paddle component and the baffle mechanism can deflect or bend under the action of force. According to the particle size of the lithium battery anode material precursor required by the process, the deflection or bending angle of the baffle mechanism or the paddle assembly is adjusted according to the particle-angle model, so that the lithium battery anode material precursors with different particle sizes are produced by changing the stirring intensity on the premise of not changing the output power of the driving motor, and the method is convenient to use, low in labor intensity, high in production efficiency and long in equipment use.

Description

Device and method for preparing lithium battery positive electrode material precursors with various particle sizes
Technical Field
The invention belongs to the technical field of lithium battery positive electrode material production, and particularly relates to a device and a method for preparing lithium battery positive electrode material precursors with various particle sizes.
Background
The lithium ion battery has the superior performances of high voltage, high energy, no memory effect and long service life, so that the lithium ion battery is unique in secondary batteries and is rapidly developed and applied. The most potential lithium ion battery positive electrode materials in the market at present mainly comprise lithium cobaltate, lithium nickel manganese cobalt, lithium manganese and lithium iron phosphate series (including lithium iron phosphate, lithium vanadium phosphate and the like).
According to the particle size of the material, the precursor of the lithium battery anode material can be roughly divided into a small particle precursor, a medium particle precursor and a large particle precursor, wherein the medium and small particle precursors are mainly baked to form a single crystal material for manufacturing a high-voltage lithium battery, and the large particle precursor is mainly baked to form a polycrystalline material for manufacturing a high-capacity lithium battery. In some cases, lithium battery precursors with different particle sizes can be mixed to improve the compaction density of the material and optimize the performance of the lithium battery cathode material.
At present, the method for preparing the lithium battery positive electrode material precursor in the industry is mainly a coprecipitation method, and two methods are generally used for preparing the lithium battery positive electrode material precursors with different particle sizes. Firstly, the dosage of the dispersing agent is introduced and changed, and the method obviously changes the composition of the precursor of the lithium battery anode material, so that the compositions of the precursors of the lithium battery anode materials with different particle sizes are different, and are not beneficial to accurate control. And secondly, the power input of the stirring equipment is changed, the mode can be realized by replacing a motor with a variable-frequency speed regulating system or adopting a plurality of motors with different rated powers or stirrers with different stirring intensities, the two schemes are high in cost, the rotating speed of the motor is frequently adjusted, adverse effects can be caused on the motor and a power supply, the labor intensity is increased when the motor or the stirrer with different power is replaced, and the production efficiency is reduced.
Disclosure of Invention
Based on the above, the invention provides a device for preparing lithium battery positive electrode material precursors with various particle sizes, so as to solve the technical problem that lithium battery positive electrode material precursors with different particle sizes are difficult to produce by using the same equipment in the prior art.
The invention also provides a method for preparing lithium battery positive electrode material precursors with various particle sizes, which is used for producing lithium battery positive electrode material precursors with different particle sizes by using the same equipment and under the same material proportion.
The technical scheme for solving the technical problems is as follows:
a device for preparing lithium battery anode material precursors with various particle sizes comprises a reaction kettle, a stirring mechanism and a baffle mechanism;
the stirring mechanism is arranged on the reaction kettle and comprises a driving motor, a stirring shaft connected to the output end of the driving motor and at least one blade component arranged on the stirring shaft; the driving motor can rotate forwards and backwards; at least one of the paddle component and the baffle mechanism can deflect or bend under the action of force.
Preferably, the paddle assembly includes a first connecting plate fixedly disposed on the stirring shaft and a first rotating plate hinged to the first connecting plate.
Preferably, a maximum deflection angle of the first rotation plate and the first connection plate can be adjusted.
Preferably, at least one side of the first connecting plate is provided with a limiting elastic part, and one end of the limiting elastic part, which is far away from the first connecting plate, is connected with the first rotating plate; the limiting elastic piece enables the first connecting plate and the first rotating plate to reach the maximum deflection angle.
Preferably, the baffle mechanism comprises at least one baffle assembly arranged on the inner wall of the reaction kettle, and the baffle assembly comprises a second rotating plate which can rotate in the direction same as or opposite to the rotating direction of the driving motor.
Preferably, the reaction kettle is provided with a cover body, and the cover body is provided with an arc-shaped sliding chute taking the orthographic projection of the rotating shaft of the second rotating plate as the center of a circle; and a shifting lever is arranged at the upper end of the second rotating plate, and the upper end of the shifting lever penetrates through the arc-shaped sliding groove and can slide in the arc-shaped sliding groove.
Preferably, the reaction vessel is provided with a jacket.
A method for preparing multiple particle size lithium battery positive electrode material precursors, comprising the steps of:
preparing base solution, metal salt solution, complexing agent and precipitator;
with the apparatus for preparing lithium battery positive electrode material precursors of various particle sizes as claimed in any one of claims 1 to 7, first adding a predetermined volume of a base solution into the reaction kettle, and then setting the turning direction of the driving motor according to the particle size of the lithium battery positive electrode material precursor, and the model of the deflection angle or the bending angle of the baffle mechanism or the blade assembly, and adjusting the deflection angle or the bending angle of the baffle mechanism or the blade assembly;
and starting the driving motor, in the stirring process, according to the technological requirements, sending the metal salt solution, the complexing agent and the precipitant solution into the reaction kettle simultaneously, carrying out synthesis reaction, and stopping feeding when the particle size meets the technological requirements, thus obtaining the lithium battery anode material precursor with one size.
Preferably, the metal salt solution is one or more of soluble nickel salt, cobalt salt, manganese salt and M salt, wherein M is one or more of Mg, Ca, Cu, Al, Ti, Ta, Nb, Zr, Mo and Zn elements.
Preferably, the complexing agent is one or more of ammonia water, salicylic acid, ammonium sulfate, ammonium chloride, ammonium nitrate, EDTA, ammonium bicarbonate and ammonium carbonate; the precipitant is one or more of sodium hydroxide, potassium hydroxide, ammonium bicarbonate and ammonium carbonate.
Compared with the prior art, the invention has at least the following advantages:
the invention provides a device for preparing lithium battery anode material precursors with various particle sizes, which comprises a reaction kettle, a stirring mechanism and a baffle mechanism, wherein the stirring mechanism comprises a driving motor, a stirring shaft and a blade assembly, and at least one of the blade assembly and the baffle mechanism can be deflected or bent under the action of force. According to the particle size of the lithium battery anode material precursor of the process requirement, the particle size of the lithium battery anode material precursor and the mapping relation between the deflection or bending angles of the baffle mechanism or the blade assembly are adjusted, so that the deflection or bending angles of the baffle mechanism or the blade assembly are adjusted, and the lithium battery anode material precursor with different particle sizes is produced by changing the stirring intensity on the premise of not changing the output power of the driving motor. By adopting the device for preparing lithium battery anode material precursors with various particle sizes, lithium battery anode materials with different particle sizes can be produced by using the same reaction kettle only by actively or passively adjusting the deflection or bending angle of the baffle mechanism or the paddle component, so that the device is convenient to use, low in labor intensity, high in production efficiency and long in equipment use.
Drawings
Fig. 1 is a schematic diagram of an apparatus 10 for preparing lithium battery positive electrode material precursors of various particle sizes according to an embodiment.
Fig. 2 is a schematic structural diagram of an embodiment of the stirring mechanism.
Fig. 3 is a schematic cross-sectional view of an apparatus 10 for preparing multiple particle size lithium battery positive electrode material precursors in one embodiment.
Fig. 4 is a perspective view of an apparatus 10 for preparing multiple particle size lithium battery positive electrode material precursors in one embodiment.
In the figure: the device for preparing the lithium battery anode material precursors with various particle sizes comprises a device 10, a reaction kettle 100, a cover body 110, an arc-shaped chute 120, a jacket 130, a stirring mechanism 200, a driving motor 210, a stirring shaft 220, a blade assembly 230, a first connecting plate 231, a first rotating plate 232, a first rotating shaft 233, a limiting elastic piece 234, a limiting stop rod 235, a baffle mechanism 300, a second rotating plate 310, a second connecting plate 320 and a shifting lever 330.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The technical solutions of the present invention will be further described below with reference to the accompanying drawings of the embodiments of the present invention, and the present invention is not limited to the following specific embodiments.
It should be understood that the same or similar reference numerals in the drawings of the embodiments correspond to the same or similar parts. In the description of the present invention, it should be understood that if there are terms such as "upper", "lower", "front", "rear", "left", "right", "top", "bottom", etc., indicating orientations or positional relationships based on the orientations or positional relationships shown in the drawings, it is only for convenience of description and simplicity of description, but does not indicate or imply that the equipment or elements referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, the terms describing the positional relationships in the drawings are only used for illustrative purposes and are not to be construed as limiting the patent, and the specific meanings of the terms will be understood by those skilled in the art according to specific situations.
In one embodiment, referring to fig. 1 and 2, an apparatus 10 for preparing lithium battery positive electrode material precursors with various particle sizes includes a reaction vessel 100, a stirring mechanism 200, and a baffle mechanism 300.
The stirring mechanism 200 is installed in the reaction kettle 100, and includes a driving motor 210, a stirring shaft 220 connected to an output end of the driving motor 210, and at least one blade assembly 230 disposed on the stirring shaft 220. The driving motor 210 can rotate forward or backward, and at least one of the paddle assembly 230 and the baffle mechanism 200 can be deflected or bent under the action of force.
In one case, the electrode rotates forward or backward, and under the reaction action of the reaction solution, the paddle assembly 230 or the baffle mechanism 300 is deflected or bent, so that the contact area between the paddle assembly 230 or the baffle mechanism 300 and the reaction solution is changed, and the stirring strength of the reaction solution is changed, so as to prepare lithium battery anode material precursors with different particle sizes.
In another case, to prepare lithium battery positive electrode material precursors with different particle sizes, according to the mapping relationship between the particle size of the lithium battery positive electrode material precursor and the deflection or bending angle of the baffle mechanism 300 or the paddle assembly 230, before starting the driving motor 210, the deflection or bending angle of the baffle mechanism 300 or the paddle assembly 230 is adjusted in advance, so as to perform stirring with different stirring strengths to prepare lithium battery positive electrode material precursors with different particle sizes.
In one embodiment, the paddle assembly 230 includes a first connection plate 231 and a first rotation plate 232, the first connection plate 231 is fixedly disposed on the stirring shaft 220, and the first rotation plate 232 is hinged to the first connection plate 231. The driving motor 210 is started, and the driving motor 210 rotates forward or backward to drive the stirring shaft 220 to rotate clockwise or counterclockwise. In the stirring process, the first rotating plate 232 rotates around the hinge shaft of the first connecting plate 231 by the reaction force of the reaction solution, so that the blade assembly 230 is deflected or bent. In one embodiment, when the driving motor 210 rotates forward, the first rotation plate 232 maintains a minimum deflection angle, for example, 0 °, with the first connection plate 231. When the driving motor 210 rotates reversely, the first rotating plate 232 rotates around the first connecting plate 231 to the maximum position to form the maximum deflection angle, so that two different stirring strengths are achieved, and two lithium battery positive electrode material precursors with different particle sizes can be prepared. Preferably, the maximum deflection angle is smaller than 90 ° so that the maximum deflection angle and the minimum deflection angle can be automatically switched when the driving motor 210 switches forward and reverse rotation.
In the above embodiment, the first rotating plate 232 is hinged to the first connection plate 231, which includes but is not limited to the following forms: the first rotating plate 232 is connected to the first connection plate 231 through a hinge, the first rotating plate 232 is connected to the first connection plate 231 through a first rotating shaft 233, the first rotating plate 232 is provided with a rotating shaft, and the first connection plate 231 is provided with a shaft sleeve which is sleeved on the rotating shaft.
In a preferred embodiment, at least one side of the first connection plate 231 is provided with a position limiting elastic member 234, and one end of the position limiting elastic member 234, which is far away from the first connection plate 231, is connected to the first rotation plate 232. The stopper elastic member 234 makes the first connection plate 231 maximally deviate from the first rotation plate 232. For example, the position limiting elastic member 234 is a metal elastic sheet or a plastic elastic sheet. When the first rotation plate 232 receives a reaction force of the reaction solution, the stopper elastic member 234 receives a bending stress and is bent, thereby deflecting the first rotation plate 232 with respect to the first connection plate 231. When the reaction force applied to the first rotation plate 232 is reduced or eliminated, the stopper elastic member 234 is reset, thereby resetting the first rotation plate 232.
In still another preferred embodiment, the maximum deflection angle of the first rotation plate 232 and the first connection plate 231 can be adjusted. For example, at least one side of the first connection plate 231 is provided with a limit stopper 235, and an included angle or a horizontal distance between the limit stopper 235 and the first rotation plate 232 can be manually adjusted. The manual adjustment of the included angle or horizontal distance between the limiting stop rod 235 and the first rotating plate 232 can be achieved by various prior arts, and will not be described herein. The stirring strength is adjusted by adjusting the maximum deflection angle between the first rotating plate 232 and the first connecting plate 231, so that the preparation requirements of lithium battery anode material precursors with various particle sizes can be met.
However, although the production of lithium battery cathode material precursors with various particle sizes can be achieved by adjusting the maximum deflection angles of the first rotating plate 232 and the first connecting plate 231, since the first rotating plate 232 and the first connecting plate 231 are located in the reaction kettle 100, a mechanism for adjusting the maximum deflection angles of the first rotating plate 232 and the first connecting plate 231 also needs to be arranged in the reaction kettle 100, and therefore, when the production of lithium battery cathode material precursors with various particle sizes is switched, the reaction kettle 100 needs to be opened, and even the lithium battery cathode material precursors with various particle sizes need to enter the reaction kettle 100 manually for adjustment, which is inconvenient to operate.
Referring to fig. 3 and 4 together, it is preferable that the stirring intensity of the reaction solution is further changed by automatically or manually adjusting the deflection angle or the bending angle of the baffle mechanism 300. For example, the baffle mechanism 300 includes at least one baffle assembly disposed on the inner wall of the reaction vessel 100, and the baffle assembly includes a second rotating plate 310, and the second rotating plate 310 can rotate in the same direction or in the opposite direction to the rotating direction of the driving motor 210.
For example, a rotating shaft or a second connecting plate 320 is disposed on the inner wall of the reaction kettle 100, and the second rotating plate 310 is hinged to the second connecting plate 320, or is rotatably disposed on the rotating shaft. When the driving motor 210 is started, under the action of the reaction solution, the second rotating plate 310 deflects towards the direction the same as the rotating direction of the driving motor 210, so as to change the stirring strength, and further produce lithium battery positive electrode material precursors with different particle sizes.
Further, in order to adjust the stirring strength of the reaction solution, the reaction kettle 100 is provided with a cover 110, and the cover 110 is provided with an arc chute 120 taking the orthographic projection of the rotating shaft of the second rotating plate 310 as the center of a circle. A shift lever 330 is disposed at an upper end of the second rotating plate 310, and an upper end of the shift lever 330 penetrates through the arc-shaped sliding groove 120 and can slide in the arc-shaped sliding groove 120.
In an embodiment, scales are disposed on the arc-shaped sliding chute 120, and the offset angle of the second rotating plate 310 can be manually adjusted by adjusting the position of the shift lever 330 in the arc-shaped sliding chute 120 and keeping the adjusted position fixed, so as to conveniently and rapidly adjust the stirring strength of the reaction solution.
In some preferred embodiments, the paddle assembly 230 and the baffle mechanism 300 can be deflected or bent simultaneously, and when the baffle mechanism 300 is at the minimum deflection angle (i.e. when the second rotating plate 310 is perpendicular to the inner wall of the reaction vessel 100), the total width of the baffle mechanism 300 is not less than 1/3 of the radius of the reaction vessel 100 and not more than 1/2 of the radius of the reaction vessel 100, so as to improve the adjustability of the stirring strength of the reaction solution. When the paddle assembly 230 is located at the minimum deflection angle, the total width of the paddle assembly is not less than 1/2 of the radius of the reaction kettle 100, so as to ensure the stirring strength.
In one embodiment, the reactor 100 is provided with a jacket 130. Preferably, the jacket 130 is connected with a thermal medium feeding and discharging pipe to provide sufficient heat during the formation of the lithium battery positive electrode material precursor. The jacket 130 is further connected with a cold medium feeding and discharging pipe so as to accelerate the cooling process after the formation of the lithium battery anode material precursor is finished.
In yet another embodiment of the present invention, a method for preparing multiple particle size lithium battery positive electrode material precursors comprises the steps of:
s01, preparing a base solution, a metal salt solution, a complexing agent and a precipitating agent.
The base solution, the metal salt solution, the complexing agent and the precipitating agent can be selected according to the actual process requirements. For example, the base solution comprises industrial alkali and ammonia water, the pH of the base solution is 11-12.5, the concentration of the ammonia water in the base solution is 5-20 g/L, and the temperature of the base solution is 40-60 ℃. The metal salt solution is one or more of soluble nickel salt, cobalt salt, manganese salt and M salt, wherein M is one or more of Mg, Ca, Cu, Al, Ti, Ta, Nb, Zr, Mo and Zn elements. Further, the metal salt solution may be one or more of sulfate, chloride, nitrate and acetate of the above elements.
The complexing agent is one or more of ammonia water, salicylic acid, ammonium sulfate, ammonium chloride, ammonium nitrate, EDTA, ammonium bicarbonate and ammonium carbonate. The precipitant is one or more of sodium hydroxide, potassium hydroxide, ammonium bicarbonate and ammonium carbonate.
S02, using the apparatus 10 for preparing lithium battery positive electrode material precursors with various particle sizes as described above, first adding a predetermined volume of a base solution into the reaction kettle 100, and then setting the rotation direction of the driving motor 210 according to the particle size of the lithium battery positive electrode material precursor and the rotation direction of the driving motor 210, and the deflection angle or bending angle model of the baffle mechanism 300 or the blade assembly 230, and adjusting the deflection angle or bending angle of the baffle mechanism 300 or the blade assembly 230.
The particle size of the lithium battery positive electrode material precursor and the turning direction of the driving motor 210, and the model of the deflection angle or the bending angle of the baffle mechanism 300 or the blade assembly 230 (hereinafter referred to as "particle-angle model") are used for establishing a scatter diagram or a broken line/curve graph according to the maximum particle size of the lithium battery positive electrode material precursor which can be obtained under the turning direction of the fixed driving motor 210 and the deflection angle or the bending angle of the baffle mechanism 300 or the blade assembly 230.
During production, according to a particle-angle model and an expected particle size of the lithium battery positive electrode material precursor, the rotation direction of the driving motor 210 and the deflection angle or the bending angle of the baffle mechanism 300 or the blade assembly 230 are searched or calculated, so that the rotation direction of the driving motor 210 and the deflection angle or the bending angle of the baffle mechanism 300 or the blade assembly 230 are adjusted, the stirring strength is changed, and lithium battery positive electrode material precursors with different particle sizes are produced.
And S03, starting the driving motor 210, feeding the metal salt solution, the complexing agent and the precipitant solution into the reaction kettle 100 simultaneously according to the technological requirements in the stirring process, performing a synthesis reaction, and stopping feeding when the particle size meets the technological requirements, so as to obtain the lithium battery positive electrode material precursor with a size.
In the above process, after the rotation direction of the driving motor 210 and the baffle mechanism 300 or the deflection angle or the bending angle of the paddle assembly 230 are determined, the lithium battery anode material precursors with different particle sizes can be produced by using the same equipment under the conditions of not changing the feeding configuration of reaction raw materials and not adding other additives, so that the use is convenient, the labor intensity is low, the production efficiency is high, and the equipment is long in use.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A device for preparing lithium battery anode material precursors with various particle sizes is characterized by comprising a reaction kettle, a stirring mechanism and a baffle mechanism;
the stirring mechanism is arranged on the reaction kettle and comprises a driving motor, a stirring shaft connected to the output end of the driving motor and at least one blade component arranged on the stirring shaft; the driving motor can rotate forwards and backwards; at least one of the paddle component and the baffle mechanism can deflect or bend under the action of force.
2. The apparatus of claim 1, wherein the paddle assembly comprises a first linkage plate fixedly disposed on the agitation shaft and a first rotation plate hingedly coupled to the first linkage plate.
3. The apparatus for making multiple particle size lithium battery positive electrode material precursors according to claim 2, wherein a maximum deflection angle of the first rotation plate and the first connection plate can be adjusted.
4. The apparatus for preparing multiple particle size lithium battery positive electrode material precursors according to claim 3, wherein at least one side of the first connection plate is provided with a limiting elastic member, and one end of the limiting elastic member, which is far away from the first connection plate, is connected with the first rotation plate; the limiting elastic piece enables the first connecting plate and the first rotating plate to reach the maximum deflection angle.
5. The apparatus according to claim 1, wherein the baffle mechanism comprises at least one baffle assembly disposed on an inner wall of the reaction vessel, the baffle assembly comprising a second rotating plate, the second rotating plate being rotatable in a direction same as or opposite to a rotation direction of the driving motor.
6. The apparatus according to claim 5, wherein the reaction vessel is provided with a cover body, and the cover body is provided with an arc-shaped chute with an orthographic projection of a rotating shaft of the second rotating plate as a circle center; and a driving lever is arranged at the upper end of the second connecting plate, and the upper end of the driving lever penetrates through the arc-shaped sliding groove and can slide in the arc-shaped sliding groove.
7. The apparatus for making multiple particle size lithium battery positive electrode material precursors according to claim 1, wherein the reaction vessel is provided with a jacket.
8. A method for preparing multiple particle size lithium battery positive electrode material precursors, comprising the steps of:
preparing base solution, metal salt solution, complexing agent and precipitator;
with the apparatus for preparing lithium battery positive electrode material precursors of various particle sizes as claimed in any one of claims 1 to 7, first adding a predetermined volume of a base solution into the reaction kettle, and then setting the turning direction of the driving motor according to the particle size of the lithium battery positive electrode material precursor, and the model of the deflection angle or the bending angle of the baffle mechanism or the blade assembly, and adjusting the deflection angle or the bending angle of the baffle mechanism or the blade assembly;
and starting the driving motor, in the stirring process, according to the technological requirements, sending the metal salt solution, the complexing agent and the precipitant solution into the reaction kettle simultaneously, carrying out synthesis reaction, and stopping feeding when the particle size meets the technological requirements, thus obtaining the lithium battery anode material precursor with one size.
9. The method according to claim 8, wherein the metal salt solution is one or more of soluble nickel salt, cobalt salt, manganese salt, and M salt, wherein M is one or more of Mg, Ca, Cu, Al, Ti, Ta, Nb, Zr, Mo, and Zn.
10. The method for preparing lithium battery positive electrode material precursors with various particle sizes according to claim 8, wherein the complexing agent is one or more of ammonia, salicylic acid, ammonium sulfate, ammonium chloride, ammonium nitrate, EDTA, ammonium bicarbonate and ammonium carbonate;
the precipitant is one or more of sodium hydroxide, potassium hydroxide, ammonium bicarbonate and ammonium carbonate.
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